Pei Miao, Zhu Xiangyu, Huang Xiaojia
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen, 361005, China.
State Key Laboratory of Marine Environmental Science, Key Laboratory of the Ministry of Education for Coastal and Wetland Ecosystem, College of the Environment and Ecology, Xiamen University, Xiamen, 361005, China.
J Chromatogr A. 2018 Jan 5;1531:13-21. doi: 10.1016/j.chroma.2017.11.030. Epub 2017 Nov 15.
Effective extraction is a key step in the determination of sulfonylurea herbicides (SUHs) in complicated samples. According to the chemical properties of SUHs, a new monolithic adsorbent utilizing acrylamidophenylboronic acid and vinylimidazole as mixed functional monomers was synthesized. The new adsorbent was employed as the extraction phase of multiple monolithic fiber solid-phase microextraction (MMF-SPME) of SUHs, and the extracted SUHs were determined by high-performance liquid chromatography with diode array detection (HPLC-DAD). Results well evidence that the prepared adsorbent could extract SUHs in environmental waters and soil effectively through multiply interactions such as boronate affinity, dipole-dipole and π-π interactions. Under the optimized extraction conditions, the limits of detection for target SUHs in environmental water and soil samples were 0.018-0.17μg/L and 0.14-1.23μg/kg, respectively. At the same time, the developed method also displayed some analytical merits including wide linear dynamic ranges, good method reproducibility, satisfactory sensitivity and low consume of organic solvent. Finally, the developed were successfully applied to monitor trace SUHs in environmental water and soil samples. The recoveries at three fortified concentrations were in the range of 70.6-119% with RSD below 11% in all cases. The obtained results well demonstrate the excellent practical applicability of the developed MMF-SPME-HPLC-DAD method for the monitoring of SUHs in water and soil samples.
有效的萃取是复杂样品中磺酰脲类除草剂（SUHs）测定的关键步骤。根据SUHs的化学性质，合成了一种以丙烯酰胺基苯硼酸和乙烯基咪唑为混合功能单体的新型整体吸附剂。该新型吸附剂用作SUHs多整体纤维固相微萃取（MMF-SPME）的萃取相，萃取的SUHs通过二极管阵列检测高效液相色谱法（HPLC-DAD）测定。结果充分证明，制备的吸附剂可通过硼酸酯亲和力、偶极-偶极和π-π相互作用等多种相互作用有效地萃取环境水体和土壤中的SUHs。在优化的萃取条件下，环境水样和土壤样品中目标SUHs的检测限分别为0.018 - 0.17μg/L和0.14 - 1.23μg/kg。同时，所建立的方法还具有一些分析优点，包括宽线性动态范围、良好的方法重现性、令人满意的灵敏度和低有机溶剂消耗。最后，所建立的方法成功应用于监测环境水样和土壤样品中的痕量SUHs。在三个加标浓度下的回收率在70.6 - 119%范围内，所有情况下相对标准偏差均低于11%。所得结果充分证明了所建立的MMF-SPME-HPLC-DAD方法在监测水样和土壤样品中SUHs方面具有出色的实际适用性。
